1-(2-Chloroethyl)-3-(dicyclopropylmethyl)urea → Rilmenidine

HRID 867079노트

반응식

HRID 867079 반응식
[CH:1]1([CH:4]([CH:12]2[CH2:14][CH2:13]2)[NH:5][C:6]([NH:8][CH2:9][CH2:10]Cl)=[O:7])[CH2:3][CH2:2]1>O>[CH:1]1([CH:4]([NH:5][C:6]2[O:7][CH2:10][CH2:9][N:8]=2)[CH:12]2[CH2:14][CH2:13]2)[CH2:3][CH2:2]1

참가 물질

3

반응물 1

HCID 988261-(2-Chloroethyl)-3-(dicyclopropylmethyl)urea

생성물 1

HCID 68712Rilmenidine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

25 g of raw urea obtained by step (a) are suspended in 150 ml of water and heated under reflux for 2 hours. After allowing the temperature of the mixture to return to room temperature, the aqueous solution is extracted with ether. The aqueous phase is separated and made alkaline by adding concentrated ammonia. The resulting precipitate is separated by suction, washed with water and dried. 11.8 g of 2-(dicyclopropylmethylamino) oxazoline are thus recovered, melting at 105°-106° C. A mixture of the latter with N-(dicyclopropylmethyl) N'-(β-chloroethyl) urea gives a decrease of the melting point.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 2 hours
  3. customto return to room temperature
  4. extractionthe aqueous solution is extracted with ether
  5. customThe aqueous phase is separated
  6. additionby adding concentrated ammonia
  7. customThe resulting precipitate is separated by suction
  8. washwashed with water
  9. customdried
  10. custom11.8 g of 2-(dicyclopropylmethylamino) oxazoline are thus recovered
  11. additionA mixture of the latter with N-(dicyclopropylmethyl) N'-(β-chloroethyl) urea
  12. customgives a decrease of the melting point

출처 및 근거

ORD 기록
ord-dc15fe349c0b4c3993036749d88684bd
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04102890

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